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Methyl iodide → 6-Bromo-1-methyl-1H-indazole-4-carbonitrile

HRID 520524
ノート
印刷プレビュー

反応式

HRID 520524 の反応式
[H-].[Na+].[Br:3][C:4]1[CH:5]=[C:6]([C:13]#[N:14])[C:7]2[CH:8]=[N:9][NH:10][C:11]=2[CH:12]=1.I[CH3:16]>O1CCCC1>[Br:3][C:4]1[CH:5]=[C:6]([C:13]#[N:14])[C:7]2[CH:8]=[N:9][N:10]([CH3:16])[C:11]=2[CH:12]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 247289186-Bromo-1H-indazole-4-carbonitrile

生成物 1

HCID 666923166-Bromo-1-methyl-1H-indazole-4-carbonitrile収率 25%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

Tetrahydrofuran (27 ml) was added to a flask containing sodium hydride (0.275 g, 6.89 mmol) and the mixture was stirred for 10 minutes at 0° C. 6-Bromo-1H-indazole-4-carbonitrile (1.39 g, 6.26 mmol) was added portionwise and the mixture was stirred for 10 mins until no further effervescence was seen. Iodomethane (0.431 ml, 6.89 mmol) was added and the mixture stirred at 0° C. for 1 h. The ice bath was removed and the flask was placed in a water bath at room temperature. The reaction remained stirring for 19 h and the mixture was then evaporated in vacuo. The residual solid purified by silica (100 g) cartridge using a gradient of ethyl acetate and cyclohexane to give the title compound as a white solid (370 mg).

後処理

  1. stirringthe mixture was stirred for 10 mins until no further effervescence
  2. stirringthe mixture stirred at 0° C. for 1 h
  3. customThe ice bath was removed
  4. customthe flask was placed in a water bath at room temperature
  5. stirringThe reaction remained stirring for 19 h
  6. customthe mixture was then evaporated in vacuo
  7. customThe residual solid purified by silica (100 g) cartridge

出典と根拠

ORDレコード
ord-ac056bc358984bb08ceac37e96badeb7
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09326987B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート